CN104495891B - A kind of preparation method of fully decentralized aluminum oxide nanoparticle - Google Patents
A kind of preparation method of fully decentralized aluminum oxide nanoparticle Download PDFInfo
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- CN104495891B CN104495891B CN201510000781.9A CN201510000781A CN104495891B CN 104495891 B CN104495891 B CN 104495891B CN 201510000781 A CN201510000781 A CN 201510000781A CN 104495891 B CN104495891 B CN 104495891B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/42—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
Present method relates to a kind of method prepared by fully decentralized aluminum oxide nanoparticle, particularly the fully decentralized aluminum oxide nanoparticle preparation method of a kind of fully decentralized α.The present invention adopts cheap raw material ferric oxide and aluminium powder, batching high energy ball mill grinds by a certain percentage, by high-energy ball milling induced oxidation reduction reaction, obtain the nano composite powder based on α-aluminum oxide and α iron, then with the iron in hydrochloric acid removal nano-complex and other impurity, high-purity α-aluminum oxide nano particle is namely obtained.The raw materials used cheapness of the present invention, processing condition are simple, simple to operate, cost is low, are convenient to amplify batch production.
Description
Technical field
The present invention relates to a kind of alumina powder jointed preparation method, is a kind of preparation method of fully decentralized aluminum oxide nanoparticle exactly, particularly a kind of preparation method of fully decentralized α-aluminum oxide nano particle.
Background technology
Aluminum oxide is the pottery that purposes is the widest, and α-aluminum oxide is the stable phase of aluminum oxide, and due to the performance of its excellence, have in a lot of fields and apply extremely widely, but it being as the shortcoming of structural ceramics, is exactly fragility.This shortcoming significantly limit alumina-ceramic and applies widely just.α-aluminum oxide nano particle prepares the excellent starting material of the brilliant pottery of aluminium oxide nano, and the brilliant pottery of aluminium oxide nano is expected to the brittleness problems solving alumina-ceramic.Simultaneously α-aluminum oxide nano particle there is corrosion-resistant, high temperature resistant, high rigidity, high strength, resistance to wear, anti-oxidant, good insulating and the feature such as surface-area is large, make it be widely used in high-tech areas such as metallurgy, chemical industry, electronics, national defence, space flight and nuclear industry.
The characteristic of α-aluminum oxide nano particle directly affects the performance of the stupalith finally prepared.For preparing nano aluminium oxide pottery, needing first to prepare dispersion soilless sticking, a aluminum oxide nanoparticle powder that particle is tiny, then carrying out shaping and densification sintering.If the dispersiveness of powder is bad, have reunion, shaping biscuit mesoporosity distribution of sizes is very wide, and in sintering densification process, gross blow hole is difficult to eliminate, and raises sintering temperature and excessive grain can be caused to grow up.Secondly, nano particle is more tiny, and under certain sintering temperature, densification rate is fast, and is expected to obtain fine and close compact grained α-aluminum oxide pottery.In electronics industry, along with multilayer wiring substrate slimming increasingly (<100nm), and require that substrate has good physical structure, this only has the ultra-fine aluminum oxide nanoparticle powder of use just can meet the demands.
So far, people have attempted multiple method and have prepared fully decentralized aluminum oxide nanoparticle powder, but not very successful, and prepare fully decentralized a aluminum oxide nanoparticle powder, and particularly the aluminum oxide nanoparticle powder of single a phase is then more difficult.The common method preparing nanometer alumina powder has the precipitator method (J.G.Li, X.D.Sun.Actamater., 2000,48,3103-3112.), spray pyrolysis (R.M.Laine, J.C.Marchal, H.P.Sun, X.Q.Pan.NatureMater., 2006,5,710-712.), microemulsion method (Y.Pang, X.Bao.J.Mater.Chem., 2002,12,3699-3704.) and sol-gel method (FeldeB.Adv.Sci.Technol., 1999,14,49-56.).Owing to preparing a aluminum oxide nanoparticle powder by these methods, generally need the calcining through more than 1000oC, make particle growth, form serious agglomeration and sintering phenomenon.Even if by the way of adding crystal seed and isolation phase, make transformation temperature be reduced to below 1000oC, sintering phenomenon still cannot be avoided, and the nanoparticle size obtained thus is large.Therefore preparation average particle size particle size a aluminum oxide nanoparticle powder that is little, dispersion soilless sticking is still a difficult problem.
Summary of the invention
The invention provides one and can overcome prior art deficiency, fully decentralized aluminum oxide nanoparticle can be prepared, particularly prepare the method for a aluminum oxide nanoparticle of fully decentralized soilless sticking.
The preparation method of fully decentralized aluminum oxide nanoparticle of the present invention is, the stoichiometry of reacting by formula 1 takes
2Al+Fe
2O
3=2Fe+Al
2O
3
Formula 1
Brown iron oxide and aluminium powder; grind in high energy ball mill; ball milling parameter during ball milling is: rotating speed is 200rpm-400rpm; ball material mass ratio 15:1-100:1; milling time is 10h-100h, adopts argon shield in mechanical milling process, then ball milling gained powder chlorohydric acid pickling is removed iron and impurity; isolate the powder after pickling again, obtain fully decentralized aluminum oxide nanoparticle.
In the preparation method of fully decentralized aluminum oxide nanoparticle of the present invention, preferred ball milling parameter is: rotating speed is 200r-300rpm, ball material mass ratio is 20:1-50:1, milling time is 20h-80h, ball milling is carried out and (namely gained powder chlorohydric acid pickling removes iron and impurity again through aftertreatment under this parameter, isolate the powder after pickling), namely obtain fully decentralized α-aluminum oxide nano particle.
The present invention's wound adopts high-energy ball milling induced oxidation reduction reaction, prepare the nano-complex of a aluminum oxide and a iron, a iron also can serve as the matrix of mixture in this course, the gathering of further prevention a aluminum oxide, subsequently by the iron in bite removal mixture and other impurity, namely obtain high-purity a aluminum oxide nanoparticle powder.Successfully solve the thick and problem of bad dispersibility of particle in the preparation of α-aluminum oxide nano particle.
The present invention adopts high-energy ball milling and bite method, do not need through high-temperature calcination, directly can prepare a aluminum oxide nanoparticle powder disperseing soilless sticking, particle tiny completely, for the preparation of aluminium oxide nano pottery and toughness thereof and Study of Superplasticity, a aluminum oxide nanoparticle are laid a good foundation in the direct application in a lot of field.
The method preparing α-aluminum oxide nano particle provided by the present invention uses cheap raw material ferric oxide and aluminium powder, the present invention due to raw materials used cheapness, processing condition simple, easy and simple to handle, have that cost is low, repeatable strong, output is large, be easy to amplify the advantages such as mass production.The α-aluminum oxide nanoparticle size obtained in the embodiment utilizing method of the present invention to prepare tiny (median size is 10.7nm, and size distribution is 3 – 77nm), disperse soilless sticking completely.If further optimized parameter in the present invention concrete enforcement, likely obtain particle size tiny and disperse the α-aluminum oxide nano particle of soilless sticking completely.
Accompanying drawing explanation
X-ray diffraction (XRD) spectrum that Fig. 1 is the mixture powder that obtains after ball milling in embodiment 1.
Transmission electron microscope (TEM) the bright field image figure of mixture powder of Fig. 2 for obtaining after ball milling in embodiment 1.
Transmission electron microscope (TEM) the dark field image figure of mixture powder of Fig. 3 for obtaining after ball milling in embodiment 1.
Fig. 4 is X-ray diffraction (XRD) spectrum of the α-aluminum oxide nano particle of preparation in embodiment 1.
Fig. 5 is transmission electron microscope (TEM) figure of the α-aluminum oxide nano particle of preparation in embodiment 1.
Fig. 6 is the EDS spectrum analysis of the α-aluminum oxide nano particle of preparation in embodiment 5.
Fig. 7 is X-ray diffraction (XRD) spectrum of the α-aluminum oxide nano particle of preparation in embodiment 6.
Fig. 8 is transmission electron microscope (TEM) figure of the α-aluminum oxide nano particle of preparation in embodiment 6.
Embodiment
Below in conjunction with embodiment, the present invention is further elaborated.
Embodiment 1
Ball grinder volume adopts 80ml, ball radius selects 10mm, ferric oxide (purity >=99.0wt.% is weighed according to stoichiometric ratio, 0.2-0.3 μm) and aluminium powder (purity >=99.0wt.%, 100-200 order), altogether 2g(wherein brown iron oxide 1.4949g, account for total mass 74.74%, aluminium powder 0.5051g, accounts for total mass 25.26%), ratio of grinding media to material is 50:1.First under master rotating speed 50rpm, by ingredients mixing 30min; Then, under master rotating speed 300rpm, by the powder ball milling 20h after Homogeneous phase mixing, in mechanical milling process, argon shield is adopted.X-ray diffraction (XRD) spectrum of ball milling gained powder and transmission electron microscope (TEM) photo are respectively as shown in Figure 1, Figure 2, Figure 3 shows.By high-energy ball milling, obtain the mixture (Fig. 1) with α-aluminum oxide and α iron composition, can find out that from transmission electron microscope (TEM) light field and details in a play not acted out on stage, but told through dialogues photo (Fig. 2, Fig. 3) tiny α-aluminum oxide nanoparticulate dispersed is in α iron-based body.
Ball milling gained powder is put into beaker, adds the hydrochloric acid of enough 12mol/L, magnetic agitation 10h, leave standstill 10h, suck supernatant liquor, retain precipitation, the hydrochloric acid rejoining enough 12mol/L repeats above-mentioned acid cleaning process three times.Residue precipitation is proceeded to centrifuge tube, and under rotating speed 10000rpm, centrifugal 5min removes the acid containing impurity.In the precipitation after above-mentioned disacidify, add the hydrochloric acid of 4mol/L, after ultrasonic disperse, centrifuge washing 5min under rotating speed 10000rpm, this eccentric cleaning process repeats once.XRD(Fig. 4) show,
Be α-aluminum oxide to product.Can find out that acid-leached product is α-aluminum oxide nano particle from TEM photo (Fig. 5), its good dispersity, particle is tiny.Through statistics, mean particle size is 10.7nm, and size distribution is 3 – 77nm.
Embodiment 2
Ball grinder volume adopts 80ml, ball radius selects 10mm, ferric oxide (purity >=99.0wt.% is weighed according to stoichiometric ratio, 0.2-0.3 μm) and aluminium powder (purity >=99.0wt.%, 100-200 order), altogether 3.3g(wherein brown iron oxide 2.4666g, account for total mass 74.74%, aluminium powder 0.8334g, accounts for total mass 25.26%), ratio of grinding media to material is 30:1.First under master rotating speed 50rpm, by ingredients mixing 30min; Then, under master rotating speed 300rpm, by the powder ball milling 40h after Homogeneous phase mixing, in mechanical milling process, argon shield is adopted.By high-energy ball milling, obtain the mixture based on α-aluminum oxide and α iron, α-aluminum oxide is evenly dispersed in α iron-based body.
Ball milling gained powder is put into beaker, adds the hydrochloric acid of enough 12mol/L, magnetic agitation 10h, leave standstill 10h, suck supernatant liquor, the hydrochloric acid rejoining enough 12mol/L repeats above-mentioned acid cleaning process three times.Residue precipitation is proceeded to centrifuge tube, and under rotating speed 10000rpm, centrifugal 5min removes the acid containing impurity.In the precipitation after above-mentioned disacidify, add the hydrochloric acid of 4mol/L, after ultrasonic disperse, centrifuge washing 5min under rotating speed 10000rpm, this eccentric cleaning process repeats once.Namely α-aluminum oxide nano particle is obtained.
Gained α-aluminum oxide nanoparticulate dispersed is good, and particle is tiny, and through statistics, mean particle size is 12.2nm, and size distribution is 2.9 – 78.2nm.
Embodiment 3
Ball grinder volume adopts 80ml, and ball radius selects 10mm, according to stoichiometric ratio
Weigh ferric oxide (purity >=99.0wt.%, 0.2-0.3 μm) and aluminium powder (purity >=99.0wt.%, 100-200 order), 2g(wherein brown iron oxide 1.4949g, accounts for total mass 74.74%, aluminium powder 0.5051g, accounts for total mass 25.26% altogether), ratio of grinding media to material is 50:1.First under master rotating speed 50rpm, by ingredients mixing 30min; Then, under master rotating speed 300rpm, by the powder ball milling 60h after Homogeneous phase mixing, in mechanical milling process, argon shield is adopted.By high-energy ball milling, obtain the mixture based on α-aluminum oxide and α iron, α-aluminum oxide is evenly dispersed in α iron-based body.
Ball milling gained powder is put into beaker, adds the hydrochloric acid of enough 12mol/L, magnetic agitation 10h, leave standstill 10h, suck supernatant liquor, the hydrochloric acid rejoining enough 12mol/L repeats above-mentioned acid cleaning process three times.Residue precipitation is proceeded to centrifuge tube, and under rotating speed 10000rpm, centrifugal 5min removes the acid containing impurity.In the precipitation after above-mentioned disacidify, add the hydrochloric acid of 4mol/L, after ultrasonic disperse, centrifuge washing 5min under rotating speed 10000rpm, this eccentric cleaning process repeats once.Namely α-aluminum oxide nano particle is obtained.
Gained α-aluminum oxide nanoparticulate dispersed is good, and particle is tiny, and through statistics, mean particle size is 14.2nm, and size distribution is 3.1 – 125nm.
Embodiment 4
Ball grinder volume adopts 80ml, ball radius selects 10mm, ferric oxide (purity >=99.0wt.% is weighed according to stoichiometric ratio, 0.2-0.3 μm) and aluminium powder (purity >=99.0wt.%, 100-200 order), altogether 5g(wherein brown iron oxide 3.7372g, account for total mass 74.74%, aluminium powder 1.2628g, accounts for total mass 25.26%), ratio of grinding media to material is 20:1.First under master rotating speed 50rpm, by ingredients mixing 30min; Then, under master rotating speed 250rpm, by the powder ball milling 40h after Homogeneous phase mixing, in mechanical milling process, argon shield is adopted.By height
Energy ball milling, obtain the nano-complex based on α-aluminum oxide and α iron, α-aluminum oxide is evenly dispersed in α iron-based body.
Ball milling gained powder is put into beaker, adds the hydrochloric acid of enough 12mol/L, magnetic agitation 10h, leave standstill 10h, suck supernatant liquor, the hydrochloric acid rejoining enough 12mol/L repeats above-mentioned acid cleaning process three times.Residue precipitation is proceeded to centrifuge tube, and under rotating speed 10000rpm, centrifugal 5min removes the acid containing impurity.In the precipitation after above-mentioned disacidify, add the hydrochloric acid of 4mol/L, after ultrasonic disperse, centrifuge washing 5min under rotating speed 10000rpm, this eccentric cleaning process repeats once.Namely α-aluminum oxide nano particle is obtained.
Gained α-aluminum oxide nanoparticulate dispersed is good, and particle is tiny, and through statistics, mean particle size is 13.5nm, and size distribution is 2.9-101nm.
Embodiment 5
Ball grinder volume adopts 80ml, ball radius selects 10mm, ferric oxide (purity >=99.0wt.% is weighed according to stoichiometric ratio, 0.2-0.3 μm) and aluminium powder (purity >=99.0wt.%, 100-200 order), altogether 5g(wherein brown iron oxide 3.7372g, account for total mass 74.74%, aluminium powder 1.2628g, accounts for total mass 25.26%), ratio of grinding media to material is 20:1.First under master rotating speed 50rpm, by ingredients mixing 30min; Then, under master rotating speed 300rpm, by the powder ball milling 20h after Homogeneous phase mixing, in mechanical milling process, argon shield is adopted.Bring out thermite reaction by high-energy ball milling, obtain the nano-complex based on α-aluminum oxide and α iron, α-aluminum oxide is evenly dispersed in α iron-based body.
Ball milling gained powder is put into beaker, adds the hydrochloric acid of enough 12mol/L, magnetic agitation 10h, leave standstill 10h, suck supernatant liquor, the hydrochloric acid rejoining enough 12mol/L repeats above-mentioned acid cleaning process three times.Residue precipitation is proceeded to centrifuge tube, at rotating speed 10000
Under rpm, centrifugal 5min removes the acid containing impurity.In the precipitation after above-mentioned disacidify, add the hydrochloric acid of 4mol/L, after ultrasonic disperse, centrifuge washing 5min under rotating speed 10000rpm, this eccentric cleaning process repeats once.Namely α-aluminum oxide nano particle is obtained.
Gained α-aluminum oxide nanoparticulate dispersed is good, and particle is tiny, and through statistics, mean particle size is 14.3nm, and size distribution is 2-250nm.
EDS spectrum (Fig. 6) analyzes containing C, Cu, O, Al and Fe element in show sample, and wherein C, Cu element is from preparing sample for use in transmitted electron microscope plating carbon supporting film used, and composition analysis is as shown in the table.This explanation almost can remove the ferro element in sample by pickling, the purity obtaining α-aluminum oxide is that 99.4wt%(material purity is only 99%).
Embodiment 6
Adopt 500ml ball grinder, ball radius selects 10mm, 20mm mutually to arrange in pairs or groups, ferric oxide (purity >=99.0wt.% is weighed according to stoichiometric ratio, 0.2-0.3 μm) and aluminium powder (purity >=99.0wt.%, 100-200 order), altogether 6g(wherein brown iron oxide 4.4846g, account for total mass 74.74%, aluminium powder 1.5154g, accounts for total mass 25.26%), ratio of grinding media to material is 50:1.First under master rotating speed 50rpm, by ingredients mixing 30min; Then, under master rotating speed 300rpm, by the powder ball milling 20h after Homogeneous phase mixing, in mechanical milling process, argon shield is adopted.By high-energy ball milling, obtain the nano-complex based on α-aluminum oxide and α iron, α-aluminum oxide is evenly dispersed in α iron-based body.
Ball milling gained powder is put into beaker, adds the hydrochloric acid of enough 12mol/L, magnetic agitation 10h, leave standstill 10h, suck supernatant liquor, rejoin enough 12mol/L's
Hydrochloric acid repeats above-mentioned acid cleaning process three times.Residue precipitation is proceeded to centrifuge tube, and under rotating speed 10000rpm, centrifugal 5min removes the acid containing impurity.In the precipitation after above-mentioned disacidify, add the hydrochloric acid of 4mol/L, after ultrasonic disperse, centrifuge washing 5min under rotating speed 10000rpm, this eccentric cleaning process repeats once.XRD(Fig. 7) show, obtaining product is α-aluminum oxide nano particle.
Can find out that gained α-aluminum oxide nanoparticulate dispersed is good from TEM photo (Fig. 8), particle is tiny, and through statistics, mean particle size is 10.8nm, and size distribution is 3.4 – 78.4nm.
, there is not too large change because of dilatation, improve the efficiency preparing α-aluminum oxide nano particle simultaneously in α-aluminum oxide nanoparticle size and dispersiveness, provides possibility for amplifying batch production α-aluminum oxide nano particle.
Claims (1)
1. a preparation method for fully decentralized aluminum oxide nanoparticle, the stoichiometric ratio of reacting by formula 1 takes brown iron oxide and aluminium powder, grinds, in mechanical milling process in high energy ball mill
2Al+Fe
2O
3=2Fe+Al
2O
3
Formula 1
Adopt argon shield; again ball milling gained powder chlorohydric acid pickling is removed iron and impurity; isolate the powder after pickling again; obtain fully decentralized aluminum oxide nanoparticle; it is characterized in that, ball milling parameter is: rotating speed is 200r-300rpm, and ball material mass ratio is 20:1-50:1; milling time is 20h-80h, obtains fully decentralized α-aluminum oxide nano particle through aftertreatment.
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| CN106044809B (en) * | 2016-05-27 | 2018-10-26 | 兰州大学 | A kind of preparation method being completely dispersed alpha-aluminium oxide nano particle |
| CN109093124B (en) * | 2017-06-21 | 2020-11-27 | 北京大学 | Method for preparing metal nano material by high-energy ball milling reduction method |
| CN115818689A (en) * | 2022-12-30 | 2023-03-21 | 深圳市晖耀电子有限公司 | Nanocrystalline alpha-Al 2 O 3 Powder preparation method |
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| CN1288861A (en) * | 2000-08-25 | 2001-03-28 | 山东省海洋化工科学研究院 | Method for preparing metal oxide nano material |
| CN103435095A (en) * | 2013-08-14 | 2013-12-11 | 西安工程大学 | Method for preparing nano tin dioxide/composited nano tin dioxide through high-energy ball milling method |
| CN104070171A (en) * | 2014-06-12 | 2014-10-01 | 陕西斯瑞工业有限责任公司 | Preparation method for superfine chromium powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1288861A (en) * | 2000-08-25 | 2001-03-28 | 山东省海洋化工科学研究院 | Method for preparing metal oxide nano material |
| CN103435095A (en) * | 2013-08-14 | 2013-12-11 | 西安工程大学 | Method for preparing nano tin dioxide/composited nano tin dioxide through high-energy ball milling method |
| CN104070171A (en) * | 2014-06-12 | 2014-10-01 | 陕西斯瑞工业有限责任公司 | Preparation method for superfine chromium powder |
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